Process of producing ice colors on cotton



Patented Aug. 9, 1927.

UNITED STATES.

KABLJELLINOK AND wHiHELH L'HB-IBT,

or orrnmon-on-m-mnn, onmrm,

ABBIGNOBS TO I. G. FABBENINDUSTRIE AKTIENGESELLSCHAFT, OI FRANKFURT-onrnn mm, (mm; 1

PROCESS OF PRODUCING ICE COLORS ON COTTON.

Ho Drawing. Application Med January 15, 1925,

When developing ice colors with non-acid, that is neutral or with sodaalkaline diazo solutions there is the danger of a progressivedecomposition of the diazo compound, produced by. the alkaline solution,which together with the padded material is put into the dye-bath, makingit alkaline with caustic alkali, so that unsatisfactory feeble ortroubled or nonuniform dyeings are liable to be obtained. Thisinconvenience comes especiall to light in dyeing in a standing bath andin the case of tetrazo compounds, so that it was hitherto diificult toobtain according to this method with diazo solutions uniform lotscertain to be satisfactory.

Now we have found that the injurious action of the caustic alkali uponthe diazo compound can be overcome by adding to the diazo-bathsubstances that will neutralize the alkali of the padding solutionwithout acidifying the bath, such as for example an alkaline bicarbonateor a suitable'metal salt (such as magnesium sulfate or zinc chloride) orboth together. 1

According to this method the diazo-baths remain free of products ofdecomposition,

giving uniform and clear dyeings.

The following examples illustrate the invention. r

Example 1.

The cotton goods are padded with a sclution containing gr.;of theera-chloroanilide of 2.3-oxynaphthoic aci cc. of Turkey rcd oil, 15 cc.of caustic soda solution of 34 B. and 10 cc. of formaldehydeof 30%standard in the liter, well wrung out and developed in a diazo solutionof meta-xylidin. The diazo solution" is prepared as follows: 2.5 gr. ofmeta-xylidin are mixed with 5 cc. of hydrochloric acid of B. anddissolved in cc. ofhot water. After cooling down the solution is pouredwhile stirring into a solution, cooled with ice, of 1.5 gr. of sodiumnitrite of 98% standard. The diazotation is finished in 10 minutes. Thensoda is added until the solution begins to show an alkaline reaction andthen 5 gr. of sodium bicarbonate are added.

In this manner bluish red shades are ob tsliined. The dyeing-bathremains completely c ear.

Serial No. 2,808, and in Germany February 25, 1924.

Ewamplc 2.

ATM cotton goods are padded with a solution, containing 12 gr. of theanilide of 2.3- oxynaphthoic acid, 15 cc. of Turkey red oil, 18 cc. ofcaustic soda solution of 34 B. and 12 cc. of formaldehyde, well wrungout and developed with a diazo solution of 4.4.-diaminodiphenylamine.This diazo solution is prepared as follows: 4 of 4.4:-diamidodiphenylamine are dissofi ed in 20 cc. of hot water. Aftercooling down 50 cc. of .cold water and 20 gr. of ice and 10 cc. ofhydrochloric acid of 20 B. are added. Then slowly while stirringcontinuously a solutionof 3 gr. of sodium nitrite in 5 cc. "of water ispoured in. After 10 minutes the diazo-solution is neutralized with chalkand 5 gr. of magnesium sulfate are added. 7

Dark black shades are obtained. The dye-bath is neutral after thedevelopment.

Esme s.

The cotton goods are padded with a solution, containing 3 gr. of thealpha-nu hthalide of 2.3-oxynaphthoic acid, 6' cc. 0 Turkey red oil, 9cc. of caustic soda solution of 34 B. and 3 cc. of formaldehyde ofstandard in the liter, and well desiccated. Then the cotton is developedin portions of kg. in 1000 liters ofa diazo solution of dianisidine. Forthe first 50 kg. of padded cotton the following diazo solution may beprepared: 1.2 kg. of dianisidine are dissolved with 1.05 liters ofhydrochloric acid of 20 B. in 25' liters of boiling water. Af er coolingdown 15 k". of ice, 10 liters. of water and .95 liter of ydrochloricacid of 20 B6. are added. Into this solutionslowly whilestirringcontinuously .7 kg. of sodium nitrite of 98% standard, dissolvedin 1 liter of water are poured. The diazo solution is neutralized withchalk, made up to 1000 liters and .8 kg. of zinc chloride and 10 ofsodium bicarbonate are added.

For each following lot of 50 kg. of cotton goods an addition to the bathis to be made, prepared as follows: .45 kg. of dianisidine arediazotized in the above described manner and neutralized. To this diazosolution .2 k of zinc chloride and 2 of sodium bicar nate are added.

In this manner dark blue shades are obtained. The lots, dyed one afterthe other, are uniform and the dye hath remains in a good state.

5 Now what we claim and desire to secure by Letters Patent, is thefollowing:

1. In the process of producing 1ce colors on cotton, the improvementwhich consists inusing non-acid diazo solutions and, for 10 the purposeof avoiding lean or nonuniform dycings, adding to these diazo solutionssubstances that will neutralize the alkali of ihelfmdding solutionWithout acidifying the 2. Cotton materials dyed according to claim 1.

In testimony, that we claim the foregoing as our invention, we havesigned our names, this 31st day of December 1924.

om. ING. KARL JELLINGK. DR. WILHELM CHRIST.

In this manner dark blue shades are obstances that will neutralize thealkali of tained. The lots, dyed one after the other, the paddingsolution Without acidifying the are uniform and the dye-bath remains inbath.

a good state. Cotton materials dyed according to 15 Now what we claimand desire to secure claim 1. by Letters Patent, is the followmg: Intestimony, that we claim the forego- 1. In the process of producing icecolors ing as our invention, we have signed our on cotton, theimprovement whlch consists names, this 31st day of December 1924. inusing non-acid diazo solutions and, for x the purpose of avoiding leanor nonuniform DIPL. ING. KARL J ELLINCK. dyeings, adding to these diazosolutions sub- DR. WILHELM CHRIST.

CERTIFICATE OF CORRECTION.

Patent No. 1,638,12l. Granted August 9, 1927, to

KARL JELLINEK and WILHELM CHRIST.

It is hereby certified that the naineof the first mentioned patentee ofthe above numbered patent was erroneously written and printed as "KarlJellinck" whereas said name should have been written and printed as"Karl Jellinekf'; and that the said Letters Patent ehould he read withthis correction therein that the aame may conform to the record of thecaae in the Patent Office.

Signed and sealed this 6th day of September, A D. 1927.

M. J. Moore, Seal. Acting Commissioner of Patente.

CERTIFICATE OF CORRECTION.

Patent No. 1,638,121. Granted August 9, 1927, to

KARL JELLlNEK and WILHELM CHRIST.

It is hereby certified that the namerof the first mentioned patentee ofthe above numbered patent was erroneously written and printed as "KarlJellinck" whereas said name should have been written and printed as"Karl .lellinek"; and that the said Letters Patent should be read withthis correction therein that the same may conform to the record of theone in the Patent Office.

Signed and sealed this 6th day of September, A. D. 1927.

M. J. Moore, Seal. Acting Commissioner of Patents.

